Abstract: A method for the simultaneous quantitative analysis of oxygenates, benzene and toluene in gasoline was developed by gas chromatography-mass chromatogram(GC/MS). The GC separation was performed on a quartz capillary(0.25 μm×0.25 mm×60 m) column with Ar at the flow rate of 0.65 mL•min^-1. Selected ion monitoring mode and mass chromatogram were used for the quantitative detection of oxygenates, benzene and toluene in gasoline. An internal standard method was used for the quantification with butanone(MEK) and ethylene glycol dimetnyl ether(DME) as the double internal standard. For 15 components, the correlation coefficients of the calibration curve are greater than 0.998 8, the detection limits are 2—5 mg•L^-1 and the value of recoveries are larger than 90%. Relative standard deviation of retention time is less than 0.5%. The area relative standard deviation is less than 11.05%.